Quartz glass deposition apparatus, method for producing quartz glass, and quartz glass

Abstract

The application provides a quartz glass deposition device, a preparation method of quartz glass and quartz glass. The quartz glass deposition device comprises a furnace body with an open bottom end formed by an upper furnace body and a lower furnace body, a deposition unit, a first torch and a second torch; the first torch and the second torch are fixed on the top of the upper furnace body; the first spraying direction of the first torch is towards the deposition substrate, and the first spraying direction and the axis of the furnace body have an included angle θ1, 20°≤θ1≤40°; the vertical distance between the end of the first torch away from the inside of the furnace body and the axis is 20-45 mm; the second spraying direction of the second torch is towards the deposition substrate, and the second spraying direction and the first spraying direction have an included angle θ2, 30°≤θ2≤60°. The quartz glass deposition device can be used to obtain a large-size quartz glass mass.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of optical quartz glass manufacturing, in particular to a quartz glass deposition device, a preparation method of quartz glass and quartz glass. BACKGROUND

[0002] At present, chemical vapor deposition (CVD) is the main process for preparing quartz glass. During preparation, hydrogen, oxygen and silicon-containing compounds are allowed to react at high temperature in a reaction chamber to form silica particles, which are then deposited on a deposition surface to form a quartz glass ingot. However, it is currently difficult to obtain large-size quartz glass ingots, which affects the subsequent processing of quartz glass and thus affects the application of quartz glass. SUMMARY

[0003] The present application provides a quartz glass deposition device which can be used to obtain large-size quartz glass ingots, facilitating the subsequent processing of quartz glass and broadening the application scenarios of quartz glass.

[0004] The present application provides a deposition method of quartz glass, which uses the above-mentioned quartz glass deposition device and can obtain large-size quartz glass ingots, thereby expanding the application scenarios of quartz glass.

[0005] The present application provides a quartz glass prepared by the above-mentioned preparation method, which has a large size and can be applied to more scenarios.

[0006] The present application provides a quartz glass deposition device, which comprises an upper furnace body, a lower furnace body, a deposition unit, a first torch and a second torch.

[0007] The side wall of the furnace body has exhaust holes.

[0008] The deposition unit comprises a support rod located inside the furnace body and a deposition substrate fixedly connected to the top of the support rod, wherein the support rod rotates along its own axis.

[0009] The first torch and the second torch are fixed to the top of the upper furnace body. The first torch has a first jet direction towards the deposition substrate, and the first jet direction has an included angle θ1 with the axis of the furnace body, 20°≤θ1≤40°. The vertical distance between the end of the first torch away from the interior of the furnace body and the axis is 20-45mm. The second torch has a second jet direction towards the deposition substrate, and the second jet direction has an included angle θ2 with the first jet direction, 30°≤θ2≤60°.

[0010] The quartz glass deposition device as described above, wherein the support rod drives the deposition substrate to reciprocate along the depth direction of the furnace body; and / or,

[0011] The quartz glass deposition device as described above further comprises a viewing port arranged on the sidewall of the furnace body.

[0012] The present application provides a method for preparing quartz glass, wherein the quartz glass is prepared by using the quartz glass deposition device as described above, and the method comprises the following steps:

[0013] The first torch is used to spray and burn hydrogen and oxygen, and the second torch is used to spray and burn hydrogen and oxygen, and the interior of the furnace body is preheated at the same time;

[0014] The gas circulation is formed in the interior of the furnace body by taking in gas through the bottom opening and discharging gas through the exhaust hole;

[0015] The raw material containing at least a silicon-containing compound is fed into the feeding pipe of the first torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the first torch to generate silica particles and deposit onto the deposition substrate; the raw material containing at least a silicon-containing compound is fed into the feeding pipe of the second torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the second torch to generate silica particles and deposit onto the deposition substrate;

[0016] The silica particles are deposited on the deposition substrate to form a quartz glass ingot, wherein, during the deposition process, the support rod drives the deposition substrate to rotate.

[0017] The method for preparing quartz glass as described above, wherein the raw material further comprises a titanium-containing raw material.

[0018] The method for preparing quartz glass as described above, wherein, in the raw material, the volume ratio of the silicon-containing raw material to the titanium-containing raw material is (3-7):1.

[0019] The method for preparing quartz glass as described above, wherein, in the preheating process, the flow rate of hydrogen in the first torch is 100-500 L / min, and the flow rate of oxygen is 80-300 L / min;

[0020] The flow rate of hydrogen in the second torch is 100-300 L / min, and the flow rate of oxygen is 40-160 L / min; and / or,

[0021] After the preheating process, the temperature of the furnace body is 1300-1400℃,

[0022] The raw material is fed into the first torch, and the flow rate of the raw material in the first torch is 20-40 L / min;

[0023] The second torch is connected with the raw material, and the flow rate of the raw material in the second torch is 5-10 L / min.

[0024] The preparation method as described above, wherein, after the raw material is introduced, the flow rate of hydrogen and oxygen in the first torch is adjusted, and the flow rate of hydrogen and oxygen in the second torch is adjusted, so that the temperature of the furnace body is 1500-1600℃.

[0025] The preparation method as described above, wherein, after the raw material is introduced, the flow rate of hydrogen in the first torch is 200-450 L / min, and the flow rate of oxygen is 100-270 L / min.

[0026] The flow rate of hydrogen in the second torch is 260-350 L / min, and the flow rate of oxygen is 150-200 L / min.

[0027] The preparation method as described above, wherein, during the deposition process, the vertical distance from the top of the upper furnace body to the quartz glass ingot is 200-400 mm; and / or,

[0028] The rotation speed of the deposition substrate is 12-20 r / min; and / or,

[0029] During the deposition process, the support rod drives the deposition substrate to move downward along the depth direction of the furnace body.

[0030] The present application provides a quartz glass, wherein the preparation method as described above is used.

[0031] The deposition device of the quartz glass of the present application comprises an upper furnace body, a lower furnace body, a deposition unit, a first torch and a second torch, wherein the first torch and the second torch are arranged at a certain angle with respect to the central axis of the furnace body, and the temperature in the furnace can reach the melting transition temperature of the raw material of the quartz glass, so that large-size quartz glass ingots can be produced.

[0032] The preparation method of the quartz glass provided by the present application can produce large-size quartz glass ingots, for example, a quartz glass ingot with a maximum size of φ650*1500 mm can be produced, and is widely used in the field of reflective optics.

[0033] The quartz glass provided by the present application is prepared by the preparation method of the quartz glass described above, has a large size, is suitable for various processing technologies, and has a wide range of applications. BRIEF DESCRIPTION OF DRAWINGS

[0034] In order to make the technical solutions in the embodiments of the present application or the related art clearer, the accompanying drawings needed to be used in the description of the embodiments of the present application or the related art are briefly introduced. Obviously, the accompanying drawings in the following description only show some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0035] Figure 1 The structure schematic diagram of the quartz glass deposition device in some embodiments of the present application.

[0036] Label explanation:

[0037] 1: first torch;

[0038] 2: second torch;

[0039] 3: observation port;

[0040] 4: upper furnace body;

[0041] 5: lower furnace body;

[0042] 6: deposition base;

[0043] 7: support rod;

[0044] 8: exhaust hole;

[0045] 9: bottom opening. DETAILED DESCRIPTION

[0046] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all the other embodiments obtained by those skilled in the art without any creative effort belong to the protection scope of the present application.

[0047] The first aspect of the present application provides a quartz glass deposition device, comprising: an upper furnace body, a lower furnace body connected to each other to form a furnace body with a bottom opening, a deposition unit, a first torch and a second torch;

[0048] The side wall of the furnace body has an exhaust hole;

[0049] The deposition unit comprises a support rod inside the furnace body and a deposition base fixedly connected to the top of the support rod, wherein the support rod rotates along its own axis;

[0050] The first torch and the second torch are respectively fixed on the top of the upper furnace body; the first spraying direction of the first torch is towards the deposition substrate, and the first spraying direction has an angle θ1 with the axis of the furnace body, 20°≤θ1≤40°, and the vertical distance between the end of the first torch away from the inside of the furnace body and the axis is 20-45mm; the second spraying direction of the second torch is towards the deposition substrate, and the second spraying direction has an angle θ2 with the first spraying direction, 30°≤θ2≤60°.

[0051] The upper furnace body of the present application has a first accommodating cavity, which comprises a sealing end and an open end arranged oppositely; the lower furnace body has a second accommodating cavity, which comprises a first open end and a second open end arranged oppositely; the open end of the upper furnace body and the first open end of the lower furnace body are connected in size, so that the first accommodating cavity of the upper furnace body and the second accommodating cavity of the lower furnace body are connected to each other to form the inside of the furnace body, and the shell of the first accommodating cavity and the shell of the second accommodating cavity constitute the side wall of the furnace body, and the second open end forms the bottom opening of the furnace body.

[0052] The present application does not limit the connection mode of the upper furnace body and the lower furnace body. The upper furnace body and the lower furnace body can be integrally formed or assembled.

[0053] In the present application, the exhaust hole is used to exhaust the gas in the inside of the furnace body. The air from the outside environment continuously enters the inside of the furnace body through the bottom opening, and the gas flows along the inner wall of the furnace body and then is exhausted through the exhaust hole, so as to ensure the temperature and the stable flow of the gas in the inside of the furnace body, and realize the stability of the gas field and the temperature field.

[0054] The present application does not limit the position of the exhaust hole, as long as it is located on the side wall of the furnace body. Specifically, the exhaust hole can be arranged on the side wall of the upper furnace body or the side wall of the lower furnace body, for example, on the side wall of the lower furnace body close to the upper furnace body.

[0055] The number of exhaust holes can be one or more. When the number of exhaust holes is two, the two exhaust holes are symmetrically arranged along the axis of the furnace body.

[0056] In the present application, the deposition unit comprises a support rod and a deposition substrate connected to the top of the support rod. The support rod is used to drive the deposition substrate to move, and the deposition substrate is used to receive the silicon dioxide particles.

[0057] The present application does not limit the mounting mode of the support rod and the deposition substrate, as long as the support rod can drive the deposition substrate at the top to rotate. Preferably, the deposition substrate is vertically mounted on the top of the support rod, and the axes of the support rod and the deposition substrate are located in the same position.

[0058] The present application does not limit the position of the whole deposition unit inside the furnace body. To further ensure the uniform distribution of the silica particles, the deposition unit is preferably vertically extended into the furnace body from the bottom opening of the furnace body, and the axis of the support rod and the deposition substrate is consistent with the axis of the furnace body.

[0059] The present application does not limit the shape of the deposition substrate, as long as it can support the silica particles, for example, the deposition substrate surface supporting the silica particles is circular or elliptical.

[0060] In the present application, the first torch and the second torch are used to supply hydrogen, oxygen and raw materials containing silicon compounds. The first torch is used to send hydrogen, oxygen and raw materials containing silicon compounds into the furnace body to occur high-temperature reaction, and the second torch is used to send hydrogen, oxygen and raw materials containing silicon compounds into the furnace body to occur reaction. Taking the first torch as an example, specifically, the hydrogen and oxygen in the first torch are burned to produce water vapor and heat, wherein the heat is used to heat the inside of the furnace body, and the water vapor can occur high-temperature hydrolysis reaction with the raw materials containing silicon compounds to form silica particles.

[0061] The first torch and the second torch of the present application are fixed on the top of the upper furnace body. To ensure that the deposition substrate can support the silica particles formed at the outlets of the first torch and the second torch, the outlets of the first torch and the second torch are preferably extended into the furnace body, and the jet directions of the first torch and the second torch are both towards the deposition substrate, i.e. the outlets of the first torch and the second torch are opposite to the surface of the deposition substrate.

[0062] In the present application, the first torch has a first jet direction with an angle θ1 with the axis of the furnace body, 20°≤θ1≤40°, wherein the first jet direction of the first torch refers to the extension direction of the axis of the first torch itself. The vertical distance between the end of the first torch away from the inside of the furnace body and the axis refers to the vertical distance between the center position of the end of the first torch away from the inside of the furnace body and the axis, which is 20mm-45mm, for example 20mm, 25mm, 30mm, 40mm, 45mm or a range formed by any two of them. The second jet direction of the second torch refers to the extension direction of the axis of the second torch itself, and the second jet direction has an angle θ2 with the first jet direction, 30°≤θ2≤60°.

[0063] The first jet direction of the first torch and the second jet direction of the second torch form a certain angle with each other, and the first torch and the second torch are arranged away from the central axis of the furnace body, which can ensure that the temperature in the furnace reaches the melting transition temperature of the quartz glass raw material, and realizes the production of large-size quartz glass.

[0064] In addition, the first burner of the present application is offset from the axis and sprays at an angle, and the second burner is at an angle to the spraying direction of the first burner. With the support rod rotating along its axis, the silica particles gradually spread evenly under the action of centrifugal force and gravity, and are more evenly distributed, so that large-size quartz glass ingots with good structural uniformity can be prepared, thereby improving the optical uniformity of the quartz glass.

[0065] The first burner and the second burner of the present application are not limited, and each of the first burner and the second burner can be independently selected from conventional burners in the art. In an embodiment, the material inlet for the silicon-containing compound is arranged at the center of the first burner and the second burner, and the material inlets for hydrogen and oxygen are arranged around the material inlet for the silicon-containing compound.

[0066] The present application can use a driving pump to facilitate the formation of a stable circulating air flow field inside the furnace. Specifically, a driving pump can be arranged outside the furnace to pump air into the furnace or to pump air out of the furnace. In an embodiment, the driving pump is arranged outside the furnace and connected to the exhaust hole to pump air out of the furnace. The driving pump continuously pumps out the exhaust gas (unreacted water vapor, unburned hydrogen-oxygen gas, and air) in the furnace and carries out part of the heat. Due to the opening at the bottom end of the furnace and the flow of the gas, air from the external environment is continuously pumped into the furnace, thereby forming a stable circulating air flow field inside the furnace.

[0067] The number of driving pumps depends on the number of exhaust holes. When the number of exhaust holes is multiple, one driving pump can be connected to each exhaust hole.

[0068] To avoid pollution of the environment by the exhaust gas, an exhaust gas collection unit is usually arranged outside the furnace. The exhaust gas collection unit includes exhaust channels and an exhaust gas collection device. Each exhaust hole is connected to one end of an exhaust channel, the other end of the exhaust channel is connected to one end of a driving pump, and the other end of the driving pump is connected to the exhaust gas collection device.

[0069] To realize the preparation of large-size quartz glass, the support rod can be automatically raised and lowered, i.e. the support rod drives the deposition substrate to reciprocate along the depth direction of the furnace. During the deposition process, the silica particles continuously accumulate and grow on the deposition substrate. By adjusting the downward movement of the support rod along the vertical direction, large-size quartz glass with uniform deposition can be obtained. The speed of the downward movement of the support rod is determined according to the deposition rate of the silica particles.

[0070] When the silica particles accumulate on the deposition substrate, the silica particles can be melted into a glass state by heating the deposition substrate to form a quartz glass ingot. In the present application, an auxiliary heating unit is used to heat the deposition substrate. In an embodiment, the auxiliary heating unit is arranged around the periphery of the deposition substrate.

[0071] In some embodiments of the present application, an observation port can also be provided on the sidewall of the furnace body to observe the state of the quartz glass ingot in the furnace body in real time. The present application does not limit the specific position and specific number of the observation port, as long as the state of the quartz glass ingot in the furnace body can be observed in real time.

[0072] The second aspect of the present application provides a method for preparing a quartz glass, wherein the quartz glass deposition device of the first aspect is used for preparation, and the method comprises the following steps:

[0073] Hydrogen and oxygen are injected and combusted by the first torch, and hydrogen and oxygen are injected and combusted by the second torch, and the interior of the furnace body is preheated at the same time;

[0074] The gas circulation in the furnace body is formed by the air inlet through the bottom opening and the air outlet through the exhaust hole;

[0075] The raw material containing at least a silicon compound is fed into the feed pipe of the first torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the first torch to generate silica particles and deposit onto the deposition substrate; the raw material containing at least a silicon compound is fed into the feed pipe of the second torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the second torch to generate silica particles and deposit onto the deposition substrate;

[0076] The silica particles are deposited on the deposition substrate to form a quartz glass ingot, wherein, during the deposition process, the support rod drives the deposition substrate to rotate.

[0077] Before preparing the quartz glass, first, the components of the quartz glass deposition device are installed according to the corresponding positions. In order to ensure that the silica particles are deposited on the deposition substrate, the position of the support rod needs to be gradually raised, so that the vertical distance between the deposition substrate and the top of the upper furnace body is 200mm-400mm. When the support rod and the deposition substrate reach this position, the rotation function can be started, and the rotation speed of the deposition substrate is 12r / min-20r / min.

[0078] Hydrogen and oxygen are fed into the hydrogen and oxygen material inlet of the first torch, and the combustion of hydrogen and oxygen at the nozzle of the first torch can generate heat and water vapor; hydrogen and oxygen are fed into the hydrogen and oxygen material inlet of the second torch, and the combustion of hydrogen and oxygen at the nozzle of the second torch can generate heat and water vapor; the temperature in the interior of the furnace body continues to rise due to the heat generated by the combustion of hydrogen and oxygen, thereby preheating the interior of the furnace body.

[0079] In the present application, the preheating temperature is 1300-1400℃, for example, 1300℃, 1310℃, 1320℃, 1330℃, 1350℃, 1400℃ or a range consisting of any two of them.

[0080] By adjusting the flow rate of hydrogen and oxygen in the first torch and the second torch, the temperature inside the furnace body can be controlled to rise rapidly and stably, thereby preheating the inside of the furnace body. In an embodiment, during the preheating process,

[0081] In the first torch, the flow rate of hydrogen is 100-500L / min, for example, 100L / min, 200L / min, 250L / min, 300L / min, 350L / min, 400L / min, 450L / min, 500L / min or a range consisting of any two of them; the flow rate of oxygen is 80-300L / min, for example, 80L / min, 100L / min, 120L / min, 140L / min, 150L / min, 200L / min, 210L / min, 220L / min, 230L / min, 240L / min, 250L / min, 300L / min or a range consisting of any two of them;

[0082] In the second torch, the flow rate of hydrogen is 100-300L / min, for example, 100L / min, 200L / min, 250L / min, 300L / min or a range consisting of any two of them; the flow rate of oxygen is 40-160L / min, for example, 40L / min, 80L / min, 100L / min, 120L / min, 140L / min, 150L / min, 160L / min or a range consisting of any two of them.

[0083] In the present application, the heating rate of the furnace body can be controlled by adjusting the flow rate of hydrogen and oxygen in the first torch and the second torch. For example, by adjusting the flow rate of hydrogen and oxygen in the first torch and the second torch, the temperature of the furnace body can be raised to 1000-1300℃ within 10-30h.

[0084] When preheating the inside of the furnace body, air from the external environment continuously enters the inside of the furnace body through the bottom opening, while the exhaust hole exhausts, thereby ensuring the relative stability of the temperature and air circulation inside the furnace body, achieving the stability of the gas field and temperature field, and being conducive to the subsequent deposition of silica particles.

[0085] Further, a driving pump can be used to extract the exhaust gas inside the furnace body, at this time, the driving pump is connected with the exhaust hole, the hydrogen and oxygen combustion continuously generates heat, the driving pump continuously extracts the exhaust gas in the furnace body and takes out part of the heat, due to the setting of the bottom opening of the furnace body and the flow of the gas, the air in the external environment is also continuously extracted into the furnace body, so that a stable circulating air flow field is formed in the furnace body, and the temperature is maintained in the above-mentioned preheating temperature range.

[0086] When a stable circulating air flow field and temperature field are formed in the furnace body, the raw material including the silicon-containing compound is introduced into the first torch, the raw material including the silicon-containing compound and the water vapor generated by the combustion of hydrogen and oxygen have a high-temperature hydrolysis reaction at the nozzle of the first torch to form silicon dioxide particles and spray them to the deposition substrate; the raw material including the silicon-containing compound is introduced into the second torch, the raw material including the silicon-containing compound and the water vapor generated by the combustion of hydrogen and oxygen have a high-temperature hydrolysis reaction at the nozzle of the second torch to form silicon dioxide particles and spray them to the deposition substrate.

[0087] With the progress of the high-temperature hydrolysis reaction, the silicon dioxide particles continuously and continuously accumulate on the deposition substrate, accompanied by the rotation of the deposition substrate, the silicon dioxide particles are more uniformly distributed on the surface of the deposition substrate, at the same time, the silicon dioxide particles are transformed into a glass state, the uniformity of the structure is increased in the glassification process, and the quartz glass ingot product is formed. In the glassification process, the temperature of the deposition substrate is controlled to be above 1800 DEG C.

[0088] With the continuous progress of the deposition process, accompanied by the rotation of the deposition substrate, the silicon dioxide particles can also gradually spread uniformly to the outside of the deposition substrate after being transformed into a glass state, until the edge of the deposition substrate, and gradually cool and condense into a fixed type, forming a quartz glass ingot.

[0089] The present application can control the production rate of silicon dioxide particles by adjusting the flow rate of the raw material including the silicon-containing compound, thereby affecting the size of the quartz glass ingot. In some embodiments, the flow rate of the raw material in the first torch is 20-40 L / min; the flow rate of the raw material in the second torch is 5-10 L / min. The present application can improve the uniformity of the quartz glass by spraying the raw material through two torches.

[0090] In order to ensure the safety of the raw material including the silicon-containing compound, the present application can use a carrier gas to send the raw material including the silicon-containing compound into the first torch and the second torch, that is, the raw material including the carrier gas and the silicon-containing compound is introduced into the first torch, and the raw material including the carrier gas and the silicon-containing compound is introduced into the second torch, wherein the carrier gas can be at least one of oxygen, nitrogen and argon.

[0091] The application can adjust the flow rates of hydrogen and oxygen in the first torch and the flow rates of hydrogen and oxygen in the second torch after the raw material is fed in, so that the temperature of the furnace body is stabilized at 1500-1600 ℃, thereby better realizing the deposition of silicon dioxide and improving the size of the quartz glass and the safety of the deposition process.

[0092] Exemplarily, after the raw material is fed in, the flow rate of hydrogen in the first torch can be 200-450 L / min, and the flow rate of oxygen can be 100-270 L / min.

[0093] The flow rate of hydrogen in the second torch can be 260-350 L / min, and the flow rate of oxygen can be 150-200 L / min, so that the temperature of the furnace body is stabilized at 1500-1600 ℃.

[0094] As the silicon dioxide particles continuously accumulate and grow, a quartz glass ingot is formed, and the size of the quartz glass ingot in the depth direction continuously increases. The application can move the deposition substrate vertically downward, so that more silicon dioxide particles accumulate and grow to form a quartz glass ingot with a larger size.

[0095] In the application, the support rod can drive the deposition substrate to move downward along the depth direction of the furnace body. In the application, the quartz glass ingot is reprocessed, and the reprocessing includes cold processing such as edge grinding, cutting, grinding, and polishing.

[0096] In some embodiments of the application, when the raw material further includes a titanium-containing raw material, the expansion rate of the quartz glass at high temperature can be effectively reduced, and a quartz glass suitable for a variable-temperature environment in the field of reflective optics can be obtained. Especially in the deposition process using double spraying, the first torch is used for main deposition, and the second torch is used for auxiliary deposition, which not only ensures that the temperature in the furnace reaches the melting transition temperature of silicon dioxide and titanium dioxide, but also controls the uniformity and proportion of titanium doping in the quartz glass.

[0097] Further, when the volume ratio of the silicon-containing raw material to the titanium-containing raw material in the raw material is (3-7): 1, a quartz glass with excellent size, low expansion, and optical uniformity can be obtained. It can be applied to reflective optical elements in extreme ultraviolet (EUV) lithography systems in the field of semiconductors, and can be used to make optical fibers, atomic clock precursors, large telescope blank materials, etc.

[0098] The present application does not limit the specific type of silicon-containing compound, which can be a conventional silicon-containing compound in the art. In one embodiment, the silicon-containing compound can be selected from at least one of silicon-containing siloxane, alkoxide and tetrachloride, for example, the silicon-containing compound can be selected from at least one of silicon tetrachloride, organosiloxane, polysiloxane, for example, at least one of hexamethyldisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, hexamethylcyclotrisiloxane. The present application does not particularly limit the specific type of titanium-containing compound, which can be a conventional titanium-containing compound in the art. In one embodiment, the titanium-containing compound can be selected from at least one of silicon-containing siloxane, alkoxide and tetrachloride, for example, the titanium-containing compound can be titanium isopropoxide.

[0099] The present application provides a preparation method of quartz glass, which adopts a quartz glass deposition device with double torches intersecting at an angle to perform deposition treatment, so as to ensure that the temperature in the hearth reaches the melting transition temperature of the quartz glass raw material, and realizes the production of large-size quartz glass.

[0100] Specifically, the quartz glass can be prepared by using the above preparation method, and the size thereof can reach φ650*1500mm.

[0101] The third aspect of the present application provides a quartz glass, wherein the preparation method of the second aspect is used for preparation.

[0102] The quartz glass of the present application has a large size, is suitable for various processing processes, and has a wide range of applications.

[0103] The present application will be further described below through specific examples and comparative examples.

[0104] Example 1

[0105] The quartz glass deposition device of the present embodiment is shown in Figure 1 which includes a furnace body formed by sequentially connecting an upper furnace body 4 and a lower furnace body 5 along the depth direction to form a bottom opening 9, a deposition unit, a first torch 1 and a second torch 2;

[0106] The upper furnace body 4 has a first accommodating cavity, and the first accommodating cavity includes oppositely arranged sealing ends and open ends. The lower furnace body 5 has a second accommodating cavity, and the second accommodating cavity includes oppositely arranged first open ends and second open ends. The open end of the upper furnace body 4 and the first open end of the lower furnace body 5 are size-fitted and connected, so that the first accommodating cavity of the upper furnace body 4 and the second accommodating cavity of the lower furnace body 5 are mutually penetrated to form a furnace body interior. The shell of the first accommodating cavity and the shell of the second accommodating cavity constitute the side wall of the furnace body, and the second open end forms the bottom opening 9 of the furnace body.

[0107] The side wall of the lower furnace body 5 has exhaust holes 8 close to the upper furnace body 4 for discharging exhaust gas inside the furnace body; the number of the exhaust holes 8 is two, and the two exhaust holes 8 are symmetrically arranged along the axis of the furnace body, and each is connected to one end of the exhaust passage;

[0108] The deposition unit includes a support rod 7 located inside the furnace body and a deposition substrate 6 fixedly connected to the top of the support rod 7, the support rod 7 rotates along its own axis to drive the deposition substrate 6 to move, the deposition substrate 6 is used to receive silica particles, the axis positions of the support rod 7 and the deposition substrate 6 are consistent with the axis position of the furnace body, and the surface of the deposition substrate 6 for receiving silica particles is circular;

[0109] The first torch 1 and the second torch 2 are fixed to the top of the upper furnace body 4; the first torch 1 has a first spraying direction towards the deposition substrate, and the first spraying direction has an angle θ1 of 20° with the axis of the furnace body, and the vertical distance between the end of the first torch 1 away from the inside of the furnace body and the axis is 20mm; the second torch 2 has a second spraying direction towards the deposition substrate, and the second spraying direction has an angle θ2 of 40° with the first spraying direction;

[0110] During the deposition process, the deposition substrate 6 moves downward along the depth direction of the furnace body, and as the silica particles are uniformly distributed on the rotating and descending deposition substrate 6, quartz glass ingots are formed by high-temperature melting.

[0111] The preparation method of the quartz glass of the embodiment includes the following steps:

[0112] (1) The first torch and the second torch are used to spray and burn hydrogen and oxygen, and the inside of the furnace body is preheated; in the first torch, the flow rate of hydrogen is 280L / min, and the flow rate of oxygen is 135L / min; in the second torch, the flow rate of hydrogen is 180L / min, and the flow rate of oxygen is 100L / min; the preheating temperature is 1300℃;

[0113] (2) Nitrogen is used as a carrier gas, and raw materials including at least a silicon-containing compound are introduced into the first torch and the second torch, the silicon-containing compound reacts with water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the first torch and the second torch to generate silica particles and spray them to the deposition substrate; in the first torch, the flow rate of hydrogen is 400L / min, the flow rate of oxygen is 250L / min, and the flow rate of the raw materials is 28L / min; in the second torch, the flow rate of hydrogen is 300L / min, the flow rate of oxygen is 160L / min, and the flow rate of the raw materials is 5L / min; the temperature of the furnace wall is stably maintained at 1530-1525℃, the rotating speed of the support rod driving the deposition substrate is controlled at 14r / min, and the temperature of the deposition substrate is 1800℃;

[0114] The raw materials include octamethylcyclotetrasiloxane and titanium isopropoxide in a volume ratio of 4:1.

[0115] The quartz glass ingot with a size of Φ400mmx1500mm was prepared by the preparation method of Example 1. After cold processing, the quartz glass with a size of Φ340x200mm was prepared, and the optical uniformity of the quartz glass was 1.5x10 -6 The thermal expansion rate at 20-30℃ was 2.0x10 -8 / ℃.

[0116] Example 2

[0117] The quartz glass deposition device of this example has substantially the same structure as that of Example 1, except that:

[0118] The first spray direction has an angle θ1 of 30° with the axis of the furnace body, and the vertical distance between the end of the first torch 1 away from the inside of the furnace body and the axis is 35mm; the second spray direction has an angle θ2 of 50° with the first spray direction.

[0119] The preparation method of the quartz glass of this example is substantially the same as that of Example 1, except that:

[0120] The quartz glass deposition device of this example was used for preparation, and,

[0121] In step (1), the hydrogen flow rate in the first torch was 300L / min, and the oxygen flow rate was 160L / min; the hydrogen flow rate in the second torch was 200L / min, and the oxygen flow rate was 105L / min; and the preheating temperature was 1350℃.

[0122] In step (2), the hydrogen flow rate in the first torch was 450L / min, the oxygen flow rate was 270L / min, and the raw material flow rate was 35L / min; the hydrogen flow rate in the second torch was 320L / min, the oxygen flow rate was 170L / min, and the raw material flow rate was 10L / min; and the furnace wall temperature was stabilized at 1535-1540℃.

[0123] The quartz glass ingot with a size of Φ650mmx1500mm was prepared by the preparation method of Example 2. After cold processing, the quartz glass with a size of Φ600x300mm was prepared, and the optical uniformity of the quartz glass was 2.1x10 -6 The thermal expansion rate at 20-30℃ was 0.6x10 -8 / ℃.

[0124] Example 3

[0125] The quartz glass deposition device of the embodiment has substantially the same structure as that of Embodiment 1, except that:

[0126] The first jetting direction has an angle θ1 of 20° with the axis of the furnace body, and the vertical distance between the end of the first torch 1 away from the interior of the furnace body and the axis is 28 mm; the second jetting direction has an angle θ2 of 45° with the first jetting direction.

[0127] The preparation method of the quartz glass of the embodiment has substantially the same structure as that of Embodiment 1, except that:

[0128] The quartz glass is prepared by using the quartz glass deposition device of the embodiment, and

[0129] In step (1), in the first torch, the hydrogen flow rate is 195 L / min, and the oxygen flow rate is 99 L / min; in the second torch, the hydrogen flow rate is 168 L / min, and the oxygen flow rate is 89 L / min; and the preheating temperature is 1380℃.

[0130] In step (2), in the first torch, the hydrogen flow rate is 420 L / min, the oxygen flow rate is 260 L / min, and the raw material flow rate is 32 L / min; in the second torch, the hydrogen flow rate is 310 L / min, the oxygen flow rate is 165 L / min, and the raw material flow rate is 8 L / min; and the furnace wall temperature is stabilized at 1530-1535℃.

[0131] The quartz glass ingot prepared by the preparation method of Embodiment 3 has a size of Φ550mm×1500mm; after cold processing treatment of the quartz glass ingot, a quartz glass with a size of Φ470×230mm is prepared, and the optical uniformity of the quartz glass is 1.6×10 -6 The thermal expansion rate at 20℃-30℃ is 1.3×10 -8 / ℃.

[0132] Embodiment 4

[0133] The quartz glass deposition device of the embodiment has the same structure as that of Embodiment 1.

[0134] The preparation method of the quartz glass of the embodiment has substantially the same structure as that of Embodiment 1, except that:

[0135] The raw material includes octamethylcyclotetrasiloxane and titanium isopropoxide, and the volume ratio of octamethylcyclotetrasiloxane to titanium isopropoxide is 5:1.

[0136] The quartz glass ingot prepared by the preparation method of Embodiment 4 has a size of Φ450mm×1500mm; after cold processing treatment of the quartz glass ingot, a quartz glass with a size of Φ380×130mm is prepared, and the optical uniformity of the quartz glass is 0.8×10 -6The thermal expansion rate at 20-30°C is 1.1 x 10 -8 / °C.

[0137] Example 5

[0138] The quartz glass deposition device of this example has the same structure as that of Example 1.

[0139] The preparation method of the quartz glass of this example is basically the same as that of Example 1, except that:

[0140] The raw materials include octamethylcyclotetrasiloxane and titanium isopropoxide, and the volume ratio of octamethylcyclotetrasiloxane to titanium isopropoxide is 3.5:1.

[0141] The quartz glass ingot prepared by the preparation method of Example 5 has a size of Φ450mmx1500mm; after cold processing treatment of the quartz glass ingot, a quartz glass with a size of Φ390x270mm is prepared, and the optical uniformity of the quartz glass is 1.2x10 -6 The thermal expansion rate at 20-30°C is 0.4x10 -8 / °C.

[0142] Comparative Example 1

[0143] The quartz glass deposition device of this example has the same structure as that of Example 1, except that:

[0144] The first torch 1 is located at the center of the top of the upper furnace body, and the second spray direction has an included angle θ2 of 20° with the first spray direction.

[0145] The preparation method of the quartz glass of this example is basically the same as that of Example 1, except that:

[0146] The quartz glass deposition device of this example is used for preparation, and

[0147] In step (1), in the first torch, the hydrogen flow rate is 170L / min, and the oxygen flow rate is 80L / min; in the second torch, the hydrogen flow rate is 100L / min, and the oxygen flow rate is 70L / min; and the preheating temperature is 600°C.

[0148] In step (2), in the first torch, the hydrogen flow rate is 380L / min, and the oxygen flow rate is 220L / min; in the second torch, the hydrogen flow rate is 280L / min, and the oxygen flow rate is 150L / min; and the raw material flow rate is 5L / min; the maximum furnace wall temperature is 1430°C, and due to the too low temperature in the furnace, the silica and titanium dioxide particles cannot be effectively melted and converted into a glass state.

[0149] Comparative Example 2

[0150] The quartz glass deposition device of the present comparative example has substantially the same structure as that of Example 1, except that:

[0151] The first jet direction has an angle θ1 of 10° with the axis of the furnace body, and the vertical distance between the end of the first torch 1 away from the interior of the furnace body and the axis is 10 mm; the second jet direction has an angle θ2 of 30° with the first jet direction.

[0152] The preparation method of the quartz glass of the present comparative example is substantially the same as that of Example 1, except that:

[0153] The quartz glass is prepared using the quartz glass deposition device of the present comparative example, and

[0154] In step (1), in the first torch, the hydrogen flow rate is 350 L / min, and the oxygen flow rate is 180 L / min; in the second torch, the hydrogen flow rate is 230 L / min, and the oxygen flow rate is 140 L / min; and the preheating temperature is 1000℃.

[0155] In step (2), in the first torch, the hydrogen flow rate is 460 L / min, the oxygen flow rate is 280 L / min, and the raw material flow rate is 28 L / min; in the second torch, the hydrogen flow rate is 330 L / min, the oxygen flow rate is 180 L / min, and the raw material flow rate is 10 L / min; the furnace wall temperature continues to rise and is difficult to control, the quartz glass liquid continues to spread around and overflow the deposition base edge to wrap the support rod downward, and the shape cannot be fixed.

[0156] Comparative Example 3

[0157] The quartz glass deposition device of the present comparative example has substantially the same structure as that of Example 1, except that:

[0158] There is only one torch located at the center of the top of the upper furnace body.

[0159] The preparation method of the quartz glass of the present comparative example is substantially the same as that of Example 1, except that:

[0160] The quartz glass is prepared using the quartz glass deposition device of the present comparative example, and

[0161] In step (1), in the torch, the hydrogen flow rate is 262 L / min, and the oxygen flow rate is 158 L / min; and the preheating temperature is 900℃.

[0162] In step (2), in the torch, the hydrogen flow rate is 420 L / min, the oxygen flow rate is 260 L / min, and the raw material flow rate is 30 L / min; the maximum furnace wall temperature is 1450℃, there is obvious stratification in the quartz glass, the furnace temperature is low, it is difficult to completely melt the silicon dioxide and titanium dioxide particles, a large number of defects such as nodules and bubbles appear, and effective deposition molding cannot be achieved.

[0163] According to the embodiments and the comparative examples, the quartz glass with large size, high uniformity and low expansion can be prepared by using the device provided by the application.

[0164] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, but not to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A quartz glass deposition apparatus, characterized in that, The quartz glass deposition device comprises: a furnace body with an open bottom end, a deposition unit, a first torch and a second torch; wherein the side wall of the furnace body has an exhaust hole; the deposition unit comprises a support rod inside the furnace body and a deposition substrate fixed to the top of the support rod, wherein the support rod rotates along its own axis; the first torch and the second torch are respectively fixed to the top of the upper furnace body and are both arranged offset from the axis of the furnace body; the first torch has a first jet direction towards the deposition substrate, and the first jet direction has an angle θ1 with the axis of the furnace body, 20°≤θ1≤40°, and the vertical distance between the end of the first torch away from the interior of the furnace body and the axis is 20-45mm; the second torch has a second jet direction towards the deposition substrate, and the second jet direction has an angle θ2 with the first jet direction, 30°≤θ2≤60°; wherein the first torch is used as a main deposition torch, the second torch is used as an auxiliary deposition torch, and the flow rate of the raw material into the first torch is greater than that into the second torch.

2. The quartz glass deposition apparatus according to claim 1, characterized by the support rod drives the deposition substrate to reciprocate along the depth direction of the furnace body; and / or further comprising an observation port arranged on the side wall of the furnace body.

3. A method of producing quartz glass, characterized by, The quartz glass deposition device is prepared by the method comprising the following steps: combusting hydrogen and oxygen by the first torch and combusting hydrogen and oxygen by the second torch, while preheating the interior of the furnace body; forming a gas circulation in the interior of the furnace body by air inlet through the open bottom end and air outlet through the exhaust hole; feeding raw material containing silicon compound into the feed pipe of the first torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the first torch to generate silica particles and deposit onto the deposition substrate; feeding raw material containing silicon compound into the feed pipe of the second torch, and the raw material reacts with the water vapor generated by the combustion of hydrogen and oxygen at the nozzle of the second torch to generate silica particles and deposit onto the deposition substrate; the silica particles on the deposition substrate form a quartz glass ingot, wherein during the deposition process, the support rod drives the deposition substrate to rotate.

4. The production method according to claim 3, characterized by, The raw material further comprises titanium-containing raw material.

5. The preparation method according to claim 4, characterized in that, The volume ratio of silicon-containing raw material to titanium-containing raw material in the raw material is (3-7):

1.

6. The method of any one of claims 3-5, wherein, In the preheating process, the flow rate of hydrogen in the first torch is 100-500L / min, and the flow rate of oxygen is 80-300L / min; In the second torch, the flow rate of hydrogen is 100-300L / min, and the flow rate of oxygen is 40-160L / min; and / or After the preheating process, the temperature of the furnace body is 1300-1400℃; feeding the raw material into the first torch, and the flow rate of the raw material in the first torch is 20-40L / min; feeding the raw material into the second torch, and the flow rate of the raw material in the second torch is 5-10L / min.

7. The method of any one of claims 3-6, wherein, After the raw material is put into, the flow rate of hydrogen and oxygen in the first torch is adjusted, and the flow rate of hydrogen and oxygen in the second torch is adjusted, so that the temperature of the furnace body is 1500-1600℃.

8. The preparation method according to claim 7, characterized in that, After the raw material is put into, the flow rate of hydrogen in the first torch is 200-450L / min, and the flow rate of oxygen is 100-270L / min; The flow rate of hydrogen in the second torch is 260-350L / min, and the flow rate of oxygen is 150-200L / min.

9. The method of any one of claims 3-8, wherein, During the deposition process, the vertical distance from the top of the upper furnace body to the quartz glass weight is 200-400mm; and / or, The rotation speed of the deposition substrate is 12-20r / min; and / or, During the deposition process, the support rod drives the deposition substrate to move downward along the depth direction of the furnace body.

10. A quartz glass, characterized by, The preparation method is prepared by using any one of claims 3-9.

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